CN1730718A - Method for physically splash plating multilayer superhard thin film through magnetic control or unequilibrated type magnetic control - Google Patents
Method for physically splash plating multilayer superhard thin film through magnetic control or unequilibrated type magnetic control Download PDFInfo
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- CN1730718A CN1730718A CN 200510098824 CN200510098824A CN1730718A CN 1730718 A CN1730718 A CN 1730718A CN 200510098824 CN200510098824 CN 200510098824 CN 200510098824 A CN200510098824 A CN 200510098824A CN 1730718 A CN1730718 A CN 1730718A
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007747 plating Methods 0.000 title claims abstract description 11
- 239000010409 thin film Substances 0.000 title abstract description 5
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000004544 sputter deposition Methods 0.000 claims description 26
- 239000010410 layer Substances 0.000 claims description 23
- 238000010849 ion bombardment Methods 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 10
- 230000003746 surface roughness Effects 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 230000003213 activating effect Effects 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000007888 film coating Substances 0.000 claims description 5
- 238000009501 film coating Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 239000011229 interlayer Substances 0.000 claims description 3
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910033181 TiB2 Inorganic materials 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 claims description 2
- 230000004927 fusion Effects 0.000 claims 2
- 230000005856 abnormality Effects 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000003475 lamination Methods 0.000 claims 1
- 238000010301 surface-oxidation reaction Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 34
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 238000005240 physical vapour deposition Methods 0.000 description 5
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Abstract
Disclosed is a method for physically splash plating multilayer superhard thin film through magnetic control or unequilibrated type magnetic control comprising the steps of loading the article to be plated, placing in a vacuum environment, controlling by an electric heater for pre-heating, controlling voltage and temperature with high voltage power supply (HVPS), carrying out ionic bombardment in several phases, removing surface oxidation layer, employing magnetic control and non-balanced type magnetron sputtering for film-plating and cooling down on the plated article.
Description
Technical Field
The invention relates to a method for physically sputtering a multilayer laminated superhard film by using magnetron and unbalanced magnetron, in particular to a superhard film which can be applied to a large-sized workpiece and a superfine micro cutter to achieve good surface roughness and compact atomic stack.
Background
Film deposition is one of the most popular surface treatment methods at present, and can be applied to surface treatment of ornaments, tableware, tools, molds, semiconductor components and the like, and generally refers to a manufacturing process for growing a layer of homogeneous or heterogeneous material film on the surfaces of various metal materials, super-hard alloys, ceramic materials and wafer substrates so as to obtain the characteristics of beauty, wear resistance, heat resistance, corrosion resistance and the like.
Film Deposition can be divided into Physical Vapor Deposition (PVD), which is generally called Physical Vapor Deposition, and Chemical Vapor Deposition (CVD), which is generally called Chemical Vapor Deposition, depending on whether the Deposition process includes a Chemical reaction mechanism. The difference between PVD and CVD is that: PVD adsorption and desorption are physical adsorption and desorption, while CVD adsorption and desorption are chemical adsorption and desorption reactions.
The growth of thin films is a complex series of processes. The atoms that first reach the substrate must have longitudinal momentum spread before they can "adsorb" (adsorption) on the substrate. These atoms undergo the chemical reactions required to form a thin film on the substrate surface. The formed film forming atoms can do diffusion movement on the surface of the substrate, when the atoms collide with each other, the atoms are combined to form atomic groups, the atomic groups can be continuously and stably grown into 'nuclear islands' (island) after reaching a certain size, and the nuclear islands are mutually jointed to form a whole continuous film.
The existing method for manufacturing the superhard film is traditionally manufactured by arc physical deposition sputtering because the magnetic arc sputtering is used for optical coating or decorative coating with low temperature requirement and high surface smoothness, and the deposition speed of the formed film is slower than that of the arc sputtering, so the film is not usually used for forming the superhard film.
However, the method for manufacturing the superhard film has the disadvantages of high energy requirement (high voltage), long heating time, high temperature often exceeding 300 ℃, and the current commercial high-voltage power supply is subjected to stepless adjustment in the ion bombardment process, so that the voltage is difficult to be continuously adjusted and changed in use, the adhesion is low, the coating is difficult to adhere to the plated object, and the surface roughness of the plated object is large due to large deposited particles. The above method is therefore only suitable for large jobs where the surface smoothness is less important, such as drill bits or milling cutters with a diameter above 0.5 mm.
However, for the work with strict requirements on surface roughness, such as (less than 0.25 mm) ultra-fine micro-cutting tools, the method for manufacturing the ultra-hard thin film by arc physical deposition sputtering cannot meet the requirements on surface roughness.
Therefore, there are many defects and shortcomings in the prior art, and it is necessary to provide a coating method capable of effectively coating a superhard film on a small drill bit, which meets the requirement of surface roughness.
Disclosure of Invention
Therefore, the main objective of the present invention is to provide a method for physically sputtering a multi-layer laminated superhard film by using magnetron and unbalanced magnetron, which can achieve a superhard film with good surface roughness and dense atomic stack by controlling the temperature, bias voltage and surface cleaning in the furnace, and can be applied to various workpieces, including large workpieces and ultra-fine micro tools, such as a 0.1mm drill point, to advance the fabrication of ultra-fine micro precision workpieces.
To achieve the above object, the method of the present invention comprises the steps of: loading the plated object, placing the plated object in a vacuum environment, preheating the object under the control of an electric heater, controlling the voltage and the temperature by using a High Voltage Power Supply (HVPS), carrying out ion bombardment in stages, removing an oxide layer on the surface of the plated object, carrying out film coating on the plated object by using magnetron and unbalanced magnetron sputtering, cooling, and finishing the film coating operation.
In the above steps, the temperature and voltage are controlled by the high voltage power supply, and the surface cleaning is better achieved, so that the super-hard film with strong adhesive force, good surface roughness and dense atomic stack is achieved.
Compared with the prior art, the invention has the following advantages:
1. the invention can perform complete temperature control and voltage subsection control on the whole ion bombardment process through the control of the high-voltage power supply a, improve the smoothness of the plated object b and is beneficial to film plating operation.
2. The present invention can achieve a superhard film with good surface roughness and dense atomic stack by controlling the temperature, bias voltage, surface cleaning and the flow rate of the introduced gas in the furnace, so as to promote the manufacture of the superfine precision workpiece.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a block diagram of the high voltage power supply of the present invention;
FIG. 3 is a schematic view of a coating film of the present invention.
Detailed description of the invention
To facilitate a further understanding of the construction, use, and features of the invention, reference should be made to the appended drawings for a clear, concise, and exact understanding of these embodiments.
Referring to fig. 1, the method for physically sputtering a multi-layer laminated superhard film by using magnetron and unbalanced magnetron provided by the present invention comprises the following steps:
firstly, loading the plated object 1.
Secondly, the object to be plated is in a vacuum environment 2, and the vacuum environment is at least 6 multiplied by 10-3Pa~6×10-5Pa。
Thirdly, preheating 3 by controlling an electric heater to heat the plated object to 120-180 ℃.
Fourthly, ion bombardment is carried out 4: as shown in FIG. 1 and FIG. 2, a High Voltage Power Supply (HVPS) is used to control the voltage to be 200-2500V and the heating temperature to be 200-220V, and ion bombardment 4 is performed in stages to remove the oxide layer on the surface of the plated object. The high voltage power supply a includes: a phase control circuit a1, a protection and output selection circuit a2, a transformer circuit a3, a rectification circuit a4, a voltage doubling circuit a5 and a feedback protection circuit a 6; wherein,
the phase control circuit a1 is used to receive the trigger signal from the protection and output selection circuit a2 to control the conduction angle of the output.
The protection and output selection circuit a2 is used to receive the trigger signal outputted by the control circuit a1 when sensing abnormal condition, and control the output of the transformer circuit a3 according to the output selected by the user.
The transformer circuit a3 outputs a constant AC voltage source. The rectifier circuit a4 filters the ac signal output from the transformer circuit a3 to convert the power supply into a stable dc signal.
The voltage doubler circuit a5 is used to boost the input power.
The feedback protection circuit a6 is used to prevent the output voltage from being too high to cause damage.
The high voltage power supply a can provide negative bias outputs of four stages of 500V, 700V, 1100V, 1400V and the like in the ion bombardment 4 process to control the voltage in bombardment, so that the plated object can achieve surface smoothness in the process of removing impurities and burrs on the surface, and meanwhile, the adhesive force can be increased.
Fifthly, carrying out magnetic arc sputtering coating 5 on the object to be coated. As shown in fig. 1 and 3, magnetron and unbalanced magnetron sputtering are used to deposit a film on an object to be plated, and magnetron sputtering and unbalanced magnetron sputtering are mainly used for the arc sputtering. Magnetron sputtering uses a balanced magnetic arc gun to induce electromagnetic interaction and promote electrons to concentrate near the object b to increase ionization effect and sputtering rate. The unbalanced magnetron sputtering method uses an unbalanced magnetic arc gun to generate a large amount of particle concentration by utilizing the interactive collision of a positive magnetic field and a negative magnetic field, thereby accelerating the film deposition. In the magnetic arc sputtering coating process, the temperature is controlled to be between 90 and 300 ℃, and the manufacturing process comprises the following steps in sequence:
activating a balanced magnetic arc gun, sputtering a layer of metal interlayer c on the surface of the plated object b, wherein the metal interlayer c can be made of titanium or chromium, and the growing particles of the magnetic arc plating film are very tiny, so that a compact deposition stack can be formed, the surface hardness is high, the internal stress is strong, and the adhesive force of the plating film can be increased.
And (II) simultaneously activating the balanced magnetic arc gun and the unbalanced magnetic arc gun, and plating a fusing film layer d of a medium layer and a superhard film on the surface of the metal medium layer c, wherein the fusing film layer d can be made of titanium nitride or zirconium nitride, so that the deposition of the film is accelerated, and the film still has high adhesive force and hardness.
And (III) independently activating the unbalanced magnetic arc gun, and plating a specific superhard film layer e on the surface of the fused film layer d, wherein the superhard film layer e can be made of titanium carbonitride or zirconium carbonitride or titanium diboride.
And sixthly, cooling 6. in the cooling step, because the working temperature is not very high, a natural cooling method can be adopted, and other substances are not needed.
And seventhly, finishing the film coating work 7.
It can be seen from the above method that, as shown in fig. 1, 2 and 3, the present invention utilizes a high voltage power supply a (hvps) to perform complete temperature control and voltage segment control on the whole ion bombardment process, and can complete ion bombardment with a more precise and lower voltage value than the existing power supply, so that the surface of the object to be plated b is smoother, flat, and effectively reduces surface impurities and burrs, and simultaneously increases the adhesion force, so as to facilitate the film plating step. Can be applied to various workpieces, including large workpieces and even ultra-fine micro tools, such as 0.1mm drill points, etc.
The above description is only a specific description of the embodiments of the present invention, but one skilled in the art can understand that any insubstantial modifications or changes are included in the scope of the present invention, and the embodiments are not intended to limit the scope of the present invention.
Claims (13)
1. A method for physically sputtering a multilayer laminated superhard film by magnetron and unbalanced magnetron is characterized by comprising the following steps:
(1) loading the plated object;
(2) placing the plated object in a vacuum environment;
(3) preheating under the control of an electric heater;
(4) carrying out ion bombardment: controlling voltage and temperature by using a High Voltage Power Supply (HVPS), and carrying out ion bombardment in stages to remove an oxide layer on the surface of the plated object;
(5) performing film coating on the object to be coated by using magnetron and unbalanced magnetron sputtering;
(6) cooling is carried out;
(7) finishing the film coating work;
a superhard film with good surface roughness and dense atomic stack is obtained.
2. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 1, wherein the vacuum environment is 6 x 10-3Pa~6×10-5Pa。
3. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 1, wherein the preheating is performed to 120 ℃ to 180 ℃.
4. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 1, wherein the high voltage power supply comprises: the phase control circuit, the protection and output selection circuit, the transformer circuit, the rectification circuit, the voltage doubling circuit and the feedback protection circuit; wherein,
the phase control circuit is used for receiving the trigger signal of the protection and output selection circuit to control the output conducting angle;
the protection and output selection circuit receives a trigger signal which is controlled to be output when no abnormality is sensed and transmits the trigger signal to the phase control circuit, and the output of the conduction of the transformer circuit is controlled according to the output selected by a user;
a transformer circuit for outputting a fixed AC voltage source;
a rectifying circuit for filtering the AC signal output by the transformer circuit,
the power supply is changed into stable direct current;
the voltage doubling circuit is used for boosting the input power supply;
the feedback protection circuit is used for avoiding the damage caused by overhigh output voltage.
5. The magnetron and unbalanced magnetron physical sputtering method for multi-layer laminated superhard film as claimed in claim 4, wherein the high voltage power supply is capable of controlling the voltage to be 200-2500V.
6. The magnetron and unbalanced magnetron physical sputtering method for multilayer superhard film deposition according to claim 5, wherein the high voltage power supply provides negative bias outputs of 500V, 700V, 1100V, 1400V, etc. in 4 stages during ion bombardment.
7. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 4, wherein the high voltage power supply is capable of controlling the maximum heating temperature to be 200-220 ℃.
8. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 1, wherein the magnetron and unbalanced magnetron sputtering is used for coating the film sequentially comprising the following steps:
a. activating a balanced magnetic arc gun, and plating a metal interlayer on the surface of the plated object;
b. simultaneously activating a balanced magnetic arc gun and an unbalanced magnetic arc gun to plate a solution film layer of the dielectric layer and the superhard film on the surface of the metal dielectric layer;
c. and (3) independently activating the non-balanced magnetic arc gun, and plating a specific superhard film layer on the surface of the fusion film layer.
9. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 8, wherein the metal via is titanium or chromium.
10. The magnetron and unbalanced magnetron physical sputtering method for multilayer laminated superhard film as claimed in claim 8, wherein the fusion film is made of titanium nitride or zirconium nitride.
11. The magnetron and unbalanced magnetron physical sputtering method for multilayer lamination of superhard film as claimed in claim 8, wherein the superhard film layer is made of titanium carbonitride or zirconium carbonitride or titanium diboride.
12. The magnetron and unbalanced magnetron physical sputtering method for multi-layer laminated superhard film as claimed in claim 8, wherein the temperature during the coating process is controlled to be 90-300 ℃.
13. The magnetron and unbalanced magnetron physical sputtering method for multi-layer laminated superhard film as claimed in claim 8, wherein the step of cooling is performed by natural cooling.
Priority Applications (1)
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CN 200510098824 CN1730718A (en) | 2005-09-01 | 2005-09-01 | Method for physically splash plating multilayer superhard thin film through magnetic control or unequilibrated type magnetic control |
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CN 200510098824 CN1730718A (en) | 2005-09-01 | 2005-09-01 | Method for physically splash plating multilayer superhard thin film through magnetic control or unequilibrated type magnetic control |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101459120B (en) * | 2007-12-13 | 2010-08-11 | 中芯国际集成电路制造(上海)有限公司 | Method for removing interconnecting metal layer surface oxidation membrane |
CN105492652A (en) * | 2013-07-03 | 2016-04-13 | 欧瑞康表面处理解决方案股份公司特鲁巴赫 | TiB2 layers and use thereof |
CN109036706A (en) * | 2018-07-03 | 2018-12-18 | 中国科学院金属研究所 | A kind of post-processing approach improving transparent conductive film photoelectric properties |
-
2005
- 2005-09-01 CN CN 200510098824 patent/CN1730718A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101459120B (en) * | 2007-12-13 | 2010-08-11 | 中芯国际集成电路制造(上海)有限公司 | Method for removing interconnecting metal layer surface oxidation membrane |
CN105492652A (en) * | 2013-07-03 | 2016-04-13 | 欧瑞康表面处理解决方案股份公司特鲁巴赫 | TiB2 layers and use thereof |
CN109036706A (en) * | 2018-07-03 | 2018-12-18 | 中国科学院金属研究所 | A kind of post-processing approach improving transparent conductive film photoelectric properties |
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